纤维表面沉积二氧化硅薄膜对纤维树脂复合物性能的影响

doi:10.13591/j.cnki.kqyx.2023.03.002

摘要/Abstract

摘要：

目的探究纤维表面原子层沉积二氧化硅薄膜对牙科纤维树脂复合物性能的影响。方法利用原子层沉积技术(atomic layer deposition, ALD)在石英纤维表面沉积二氧化硅薄膜,制作纤维树脂复合物,分为A(未去除浸润剂)、B(去除浸润剂)、C(去除浸润剂+硅烷化)、D(去除浸润剂+ALD 600循环+硅烷化)4组,通过扫描电子显微镜、水接触角实验、吸湿性测试、CCK8实验、三点弯曲实验等检测纤维树脂复合物相关性能。结果原子层沉积二氧化硅薄膜后,石英纤维表面形态光滑,较处理前无明显改变;经ALD处理的石英纤维在硅烷化后呈疏水性。三点弯曲实验结果表明,经ALD改性的纤维树脂复合物力学性能显著提高(P<0.05)。电镜图像显示D组石英纤维与树脂基质之间具有良好的界面结合;此外,D组纤维树脂复合物表现出低吸附性、低溶解性与良好的生物相容性。结论原子层沉积技术在石英纤维表面沉积二氧化硅薄膜可显著提高牙科纤维增强树脂复合物的力学性能。

关键词: 原子层沉积, 纤维增强树脂复合物, 力学性能, 石英纤维, 二氧化硅

Abstract:

Objective To investigate the effects of fiber surface deposited with silicon dioxide films by atomic layer deposition on properties of dental fiber-reinforced composites. Methods SiO₂ films were deposited on the surface of quartz fiber by atomic layer deposition(ALD). Then the quartz fiber was used to manufacture fiber resin composites, which were divided into four groups: A(no soaking agent removal), B(soaking agent removed), C(soaking agent removed and silanization), and D(soaking agent removed, 600 ALD cycles performed and then silanization). Scanning electron microscopy, water contact angle test, hygroscopicity test, CCK8 test and three-point bending test were used to investigate the properties of fiber resin composites. Results The surface morphology of the quartz fiber treated by ALD was smooth and had no obvious change compared with that before treatment. Moreover, the quartz fiber showed hydrophobicity after silanization. The results of three-point bending test revealed that the mechanical properties of fiber-resin composites modified by ALD were significantly improved(P<0.05). When viewed by scanning electron microscopy, a good interfacial bonding could be seen between quartz fibers and the resin matrix in Group D. In addition, it was found that Group D had low absorbability, low solubility and good biocompatibility. Conclusion It is shown that deposition of SiO₂ films on the quartz fiber by ALD can significantly enhance the mechanical properties of fiber-reinforced composites.

Key words: atomic layer deposition, fiber-reinforced composite, mechanical property, quartz fiber, silicon dioxide

中图分类号:

R783.1

吕玮瑾, 王月秋, 陈虹, 舒菲, 张青红, 刘梅. 纤维表面沉积二氧化硅薄膜对纤维树脂复合物性能的影响[J]. 口腔医学, 2023, 43(3): 197-203.

LYU Weijin, WANG Yueqiu, CHEN Hong, SHU Fei, ZHANG Qinghong, LIU Mei. Effects of fiber surface deposited with silicon dioxide films on properties of fiber-reinforced composites[J]. Stomatology, 2023, 43(3): 197-203.

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组别	处理
A组	未去除浸润剂+树脂胶液
B组	去除浸润剂+树脂胶液
C组	去除浸润剂+硅烷化+树脂胶液
D组	去除浸润剂+ ALD 600循环+硅烷化+树脂胶液

组别	弯曲载荷						弯曲强度						弹性模量
组别	老化前/N		老化后/N		降低率		老化前/MPa		老化后/MPa		降低率		老化前/GPa		老化后/GPa		降低率
A组	168.45±10.98	122.47±4.99		27.30%		631.70±41.16		459.27±18.71		27.30%		38.52±4.15		25.41±3.87		34.03%
B组	200.78±6.73	131.13±6.46		34.69%		752.93±25.24		491.72±24.22		34.69%		41.93±4.09		31.73±3.37		24.33%
C组	220.73±7.95	176.59±4.63		20.00%		827.74±29.81		662.21±17.37		20.00%		46.36±6.22		41.70±4.16		10.05%
D组	252.85±9.69	220.18±9.53		12.92%		948.18±36.34		825.66±35.73		12.92%		46.40±7.21		44.63±3.07		3.81%
P	0.000	0.000				0.000		0.000				0.022		0.000

组别	m₀/g	m₁/g	m₂/g	m₃/g	m₄/g	m_d/g	WI	SL	WS
A	0.250±0.017	0.255±0.018	0.255±0.017	0.255±0.018	0.255±0.018	0.248±0.016	1.84%	0.88%	2.72%
B	0.229±0.007	0.233±0.007	0.233±0.006	0.233±0.007	0.233±0.007	0.226±0.007	1.75%	1.18%	2.93%
C	0.208±0.004	0.211±0.003	0.211±0.003	0.211±0.003	0.211±0.003	0.206±0.004	1.35%	0.87%	2.22%
D	0.222±0.006	0.225±0.007	0.225±0.007	0.225±0.007	0.224±0.007	0.220±0.007	1.17%	0.77%	1.94%